CN110218285B - 一种水性粘合剂及其制备方法 - Google Patents
一种水性粘合剂及其制备方法 Download PDFInfo
- Publication number
- CN110218285B CN110218285B CN201910385073.XA CN201910385073A CN110218285B CN 110218285 B CN110218285 B CN 110218285B CN 201910385073 A CN201910385073 A CN 201910385073A CN 110218285 B CN110218285 B CN 110218285B
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- Prior art keywords
- adhesive
- vinyl acetate
- monomer
- acrylate
- containing carboxyl
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000000853 adhesive Substances 0.000 title claims abstract description 48
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title abstract description 15
- 238000002360 preparation method Methods 0.000 title description 4
- 239000000178 monomer Substances 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 37
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical group CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims abstract description 32
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 24
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 14
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 13
- 239000000839 emulsion Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 229920000642 polymer Polymers 0.000 claims abstract description 9
- 230000001681 protective effect Effects 0.000 claims abstract description 8
- 239000003292 glue Substances 0.000 claims abstract description 6
- 238000007334 copolymerization reaction Methods 0.000 claims abstract 2
- 239000011230 binding agent Substances 0.000 claims description 22
- 229920001577 copolymer Polymers 0.000 claims description 7
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 6
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 6
- 229920002401 polyacrylamide Polymers 0.000 claims description 6
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 4
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 4
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 4
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 4
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 2
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 2
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 2
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 2
- 239000011976 maleic acid Substances 0.000 claims description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 2
- 229920000058 polyacrylate Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 2
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 claims 1
- 239000002002 slurry Substances 0.000 abstract description 38
- 238000000576 coating method Methods 0.000 abstract description 5
- 238000004537 pulping Methods 0.000 abstract description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 14
- 239000011888 foil Substances 0.000 description 10
- 239000003995 emulsifying agent Substances 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 229910052782 aluminium Inorganic materials 0.000 description 7
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 7
- 238000011161 development Methods 0.000 description 6
- 238000009775 high-speed stirring Methods 0.000 description 6
- 239000006258 conductive agent Substances 0.000 description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 4
- 239000010405 anode material Substances 0.000 description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 3
- BWYYYTVSBPRQCN-UHFFFAOYSA-M sodium;ethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- WQPMYSHJKXVTME-UHFFFAOYSA-M 3-hydroxypropane-1-sulfonate Chemical compound OCCCS([O-])(=O)=O WQPMYSHJKXVTME-UHFFFAOYSA-M 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- -1 separators Substances 0.000 description 2
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 2
- FFJCNSLCJOQHKM-CLFAGFIQSA-N (z)-1-[(z)-octadec-9-enoxy]octadec-9-ene Chemical compound CCCCCCCC\C=C/CCCCCCCCOCCCCCCCC\C=C/CCCCCCCC FFJCNSLCJOQHKM-CLFAGFIQSA-N 0.000 description 1
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 description 1
- FKOKUHFZNIUSLW-UHFFFAOYSA-N 2-Hydroxypropyl stearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(C)O FKOKUHFZNIUSLW-UHFFFAOYSA-N 0.000 description 1
- AGBXYHCHUYARJY-UHFFFAOYSA-N 2-phenylethenesulfonic acid Chemical compound OS(=O)(=O)C=CC1=CC=CC=C1 AGBXYHCHUYARJY-UHFFFAOYSA-N 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 239000004147 Sorbitan trioleate Substances 0.000 description 1
- PRXRUNOAOLTIEF-ADSICKODSA-N Sorbitan trioleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCC\C=C/CCCCCCCC)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCC\C=C/CCCCCCCC PRXRUNOAOLTIEF-ADSICKODSA-N 0.000 description 1
- IAXXETNIOYFMLW-COPLHBTASA-N [(1s,3s,4s)-4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl] 2-methylprop-2-enoate Chemical compound C1C[C@]2(C)[C@@H](OC(=O)C(=C)C)C[C@H]1C2(C)C IAXXETNIOYFMLW-COPLHBTASA-N 0.000 description 1
- LXEKPEMOWBOYRF-UHFFFAOYSA-N [2-[(1-azaniumyl-1-imino-2-methylpropan-2-yl)diazenyl]-2-methylpropanimidoyl]azanium;dichloride Chemical compound Cl.Cl.NC(=N)C(C)(C)N=NC(C)(C)C(N)=N LXEKPEMOWBOYRF-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229940119545 isobornyl methacrylate Drugs 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 229940093625 propylene glycol monostearate Drugs 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- LUZSXLWAUXSKHK-UHFFFAOYSA-M sodium;4-octadecoxy-4-oxobutanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCOC(=O)CCC([O-])=O LUZSXLWAUXSKHK-UHFFFAOYSA-M 0.000 description 1
- 235000019337 sorbitan trioleate Nutrition 0.000 description 1
- 229960000391 sorbitan trioleate Drugs 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
- H01M4/622—Binders being polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F218/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
- C08F218/02—Esters of monocarboxylic acids
- C08F218/04—Vinyl esters
- C08F218/08—Vinyl acetate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F285/00—Macromolecular compounds obtained by polymerising monomers on to preformed graft polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F293/00—Macromolecular compounds obtained by polymerisation on to a macromolecule having groups capable of inducing the formation of new polymer chains bound exclusively at one or both ends of the starting macromolecule
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
- C08F265/06—Polymerisation of acrylate or methacrylate esters on to polymers thereof
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- C—CHEMISTRY; METALLURGY
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F265/10—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of amides or imides
-
- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Cell Separators (AREA)
- Polymerisation Methods In General (AREA)
- Graft Or Block Polymers (AREA)
- Manufacturing & Machinery (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
本发明公开了一种水性粘合剂，其通过以下方法制备：(1)在保护胶的作用下，将含羧基的功能单体、醋酸乙烯单体以及丙烯酸酯单体混合进行前段共聚合形成粘合剂前段；(2)前段聚合物反应结束，加入醋酸乙烯单体进行中段聚合形成粘合剂中段；(3)待中段聚合结束，滴加预先将含羧基的功能单体、醋酸乙烯单体以及丙烯酸酯单体形成的预乳液，使反应完全形成粘合剂后段。该粘合剂能够适应高碱性环境下的制浆及涂布工艺，能适用于锂离子电池三元材料，能够稳定或调节锂离子电池三元材料浆料的pH值，具有广泛的市场应用价值。
Description
技术领域
本发明属于锂离子电池材料领域，具体涉及一种用于锂离子电池三元材料的水性粘合剂及其制备方法。
背景技术
锂离子电池是20世纪90粘度迅速发展起来的新一代二次电池，广泛用于小型便携式电子通讯产品和电动交通工具，电池材料的性能是锂电池产业中的核心环节。电池材料分为正极材料、负极材料、隔膜、电解液等。正极材料是制造锂离子电池的关键材料之一，占据电池成本的25％以上，其性能直接影响了电池的各项性能指标。
随着锂离子电池的高速发展，目前对锂离子电池的要求是制备更加轻便及更高能量密度的锂离子电池。而提高电池的能量密度的除制造工艺上的优化，提高锂离子电池正、负极材料的能量密度成了现阶段的重点。
在锂离子电池高速发展的过程中，在行业创新、协调、绿色、开放、共享五大发展理念中，国内、外研究人员对锂离子电池粘合剂水性化作了大量研究工作，CN201410731027.8、CN200910300150.3、CN108598486A等都已有大量的水性化产品的推广研究。但伴随着离子电池正极三元材料的发展，能够适应高碱性环境下的制浆及涂布工艺的水性粘合剂就成为配套三元材料的关键。但目前现有的水性粘合剂在使用过程中无法调整浆料的pH，浆料在存放过程中，随pH的变化，浆料的粘度会随之波动，影响极片涂布的一致性；另外，正极极片的集流体采用的是铝箔，其本身是两性物质，即在过酸或过碱条件下都会参与反应，放出气体，即腐蚀正极集流体。因此，现有的水性粘合剂无法满足锂离子电池对浆料的需求。
发明内容
有鉴于此，本发明致力于提供一种水性粘合剂，该水性粘合剂更适用于锂离子电池三元材料，能够稳定或调节锂离子电池三元材料浆料的pH值，能够适应于不同NCA比例的锂离子电池。
本发明提供一种水性粘合剂，通过以下方法制备，所述方法包括如下步骤：
(1)在保护胶的作用下，将含羧基的功能单体、部分醋酸乙烯单体以及丙烯酸酯单体混合进行前段聚合形成粘合剂前段；
(2)前段聚合物反应结束，加入醋酸乙烯单体进行中段聚合形成粘合剂中段；
(3)待中段聚合结束，滴加预先将含羧基的功能单体、醋酸乙烯单体以及丙烯酸酯单体形成的预乳液，使反应完全形成粘合剂后段。
在本发明的一个具体实施方式中，所述粘合剂为三段共聚物，所述粘合剂中段为醋酸乙烯聚合物；所述粘合剂前段或后段为含有羧基的功能单体、丙烯酸酯单体以及醋酸乙烯单体形成的共聚物。
在本发明的一个具体实施方式中，所述含有羧基的功能单体为含有羧基和不饱和键的化合物。
在本发明的一个具体实施方式中，所述含有羧基的功能单体包括但不限于甲基丙烯酸、丙烯酸、马来酸、衣康酸、马来酸酐等含有羧基且含有可聚合双键、三键等不饱和键的活性单体中的一种或多种。
在本发明的一个具体实施方式中，所述丙烯酸酯单体包括但不限于丙烯酸乙酯、丙烯酸丁酯、丙烯酸正/异辛酯、丙烯酸十二烷基酯、丙烯酸月桂酯、甲基丙烯酸聚乙二醇单甲醚、烯丙基聚乙二醇等软单体中的一种或多种，以及甲基丙烯酸甲酯、丙烯腈、丙烯酰胺、甲基丙烯酸羟乙酯、双丙酮丙烯酰胺、异冰片酯等硬单体中的一种或多种。
在本发明的一个具体实施方式中，所述粘合剂前段或后段中含有羧基的功能单体质量占比为5％-50％。例如，所述含有羧基的功能单体与所述共聚物的摩尔比为5％、10％、13％、15％、17％、20％、22％、25％、30％、33％、37％、40％、42％、45％、48％、50％等，优选地，所述含有羧基的功能单体质量占比为30％～50％，更优选地，所述含有羧基的功能单体质量占比为35％～40％。
在本发明的一个具体实施例中，所述粘合剂前段或后段中醋酸乙烯的质量占比为10％-40％。例如，所述粘合剂前段或后段中醋酸乙烯的质量占比为10％、12％、14％、16％、19％、21％、25％、28％、30％、33％、35％、38％或40％。优选地，所述粘合剂前段或后段中醋酸乙烯与所述共聚物的摩尔比为14％～30％；更优选地，所述粘合剂前段或后段中醋酸乙烯与所述共聚物的摩尔比为19％～25％。
本发明另一方面提供上述水性粘合剂的制备方法，其包括在保护胶的作用下，将含羧基的功能单体、醋酸乙烯单体、丙烯酸酯单体以及乳化剂、引发剂混合进行聚合反应。
在本发明的一个具体实施方式中，所述保护胶包括但不限于聚丙烯酰胺、聚丙烯酸盐、聚乙烯醇、羟乙基纤维素或羧甲基纤维素中的一种或多种。
在本发明的一个具体实施方式中，所述乳化剂为常规乳化剂与反应型乳化剂复配。
在本发明的一个具体实施方式中，所述常规乳化剂包括但不限于十二烷基硫酸钠、十二烷基苯磺酸钠、失水山梨醇三油酸酯、丙二醇单硬脂酸酯、聚氧乙烯油醇醚等中的一种或多种；所述反应型乳化剂包括但不限于乙烯基磺酸钠、甲基丙烯酸磺酸盐、苯乙烯磺酸盐、2-烯丙基醚3-羟基丙烷-1-磺酸盐等中的一种或多种。
在本发明的一个具体实施方式中，所述引发剂包括但不限于过硫酸钠、亚硫酸氢钠、过硫酸钾、过硫酸铵、维生素、过氧化苯甲酰、偶氮二异丁腈、AIBA、AIBI等中的一种或两种。
在本发明的一个具体实施方式中，所述水性粘合剂的制备方法包括：
(1)在保护胶的作用下，将含羧基的功能单体、部分醋酸乙烯单体以及丙烯酸酯单体在乳化剂作用下进行前段聚合，反应温度为40-80℃，恒温反应时间30min-480min；
(2)前段聚合物反应结束，按比例加入醋酸乙烯单体，反应温度为40-80℃，恒温反应时间30-240min；
(3)待中段聚合结束，加入预先将含羧基的功能单体、醋酸乙烯单体以及丙烯酸酯单体在乳化剂作用下制备形成的预乳液，在60min-240min滴加完毕，升高温度至60-90℃，恒温反应，使反应完全。
在本发明的一个具体实施方式中，所述步骤(1)或步骤(2)中反应温度为50-70℃。优选地，所述反应温度为60-70℃，例如所述反应温度为60℃、65℃、68℃，70℃。
在本发明的一个具体实施方式中，所述步骤(1)中反应温度为60-80℃。优选地，所述反应温度为70-80℃，例如所述反应温度为70℃、74℃、78℃，80℃。
本发明又一方面提供上述水性粘合剂在锂离子电池三元材料中的应用。
本发明提供的水性粘合剂至少具有以下有益效果之一：
本发明提供一种水性粘合剂，其通过分步制备形成三段共聚物，能够适应高碱性环境下的制浆及涂布工艺，能适用于锂离子电池三元材料，能够稳定或调节锂离子电池三元材料浆料的pH值，具有广泛的市场应用价值。
具体实施方式
下面将结合本发明的实施例，对本发明的技术方案进行清楚、完整地描述。显然，所描述的实施例仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
将3份的聚丙烯酰胺溶于反应釜中，待聚丙烯酰胺完全溶解后依次加入0.8份的乙烯基磺酸钠，30份的丙烯酸乙酯、15份的甲基丙烯酸以及5份的醋酸乙烯，升高温度至68℃，快速加入0.4份的过硫酸铵溶液，反应180min，制备前段聚合物；待反应完成后保持温度不变快速加入10份的醋酸乙烯以及0.1份的过硫酸铵溶液，保持68℃恒温反应60min，待反应完成后将30份的丙烯酸乙酯以及10份的醋酸乙烯在0.35份的十二烷基苯磺酸钠制成预乳液，将预乳液与0.3份的过硫酸铵溶液缓慢滴加，180min滴加完毕，升高温度至70℃，保温240min；即制得锂离子电池三元材料用水性粘合剂，粘合剂粘度在6000-8000cP.s，粘合剂固含量为20％。
实施例2
将实施例1制备的粘合剂40g以及水85g，缓慢搅拌5min，加入导电剂Super P 4g高速搅拌100min，然后加入188g正极三元材料(NCA811)高速搅拌100min，制得的正极三元材料浆料固含量为70％，粘度为5000cP.s浆料放置24h，浆料的粘度与pH至无明显变化，将其在铝箔上进行涂布，表观良好，无露箔及气泡生成。浆料的粘度及pH数据变化如表1所示：
表1浆料的粘度及pH数据变化
| 时间 | 0h | 1h | 4h | 24h |
| 粘度 | 5000 | 6000 | 8000 | 9200 |
| pH | 8.4 | 9 | 9.4 | 9.8 |
将188g正极三元材料在129g水中高速分散20min然后浆料静置，测试其pH值变化如表2所示：
表2高速分散后浆料的pH值变化
| 时间 | 0h | 1h | 4h | 24h |
| pH | 9.4 | 10.2 | 11.3 | 11.4 |
将表1与表2对比可知，实施例1中所制备的水性粘合剂能够稳定或调节pH值。
实施例3
本实施例中，将3份的聚丙烯酰胺溶于反应釜中，待聚丙烯酰胺完全溶解后依次加入0.8份的乙烯基磺酸钠，30份的丙烯酸丁酯、15份的甲基丙烯酸以及5份的醋酸乙烯，升高温度至68℃，快速加入0.4份的过硫酸铵溶液，反应240min，制备前段聚合物；待反应完成后保持温度不变快速加入5份的醋酸乙烯以及0.1份的过硫酸铵溶液，保持68℃恒温反应30min，待反应完成后将30份的丙烯酸丁酯、10份的醋酸乙烯以及10份的甲基丙烯酸在0.3份的十二烷基苯磺酸钠制成预乳液，将预乳液与0.3份的过硫酸铵溶液缓慢滴加，240min滴加完毕，升高温度至70℃，保温240min；即制得锂离子电池三元材料用水性粘合剂，粘合剂粘度为10000-14000cP.s，粘合剂固含为18％。
实施例4
将实施例3制备的粘合剂40g以及水85g缓慢搅拌5min，加入导电剂Super P 4g高速搅拌100min，然后加入188g正极三元材料(NCA811)高速搅拌100min，制得的正极三元材料浆料固含为70％，粘度为5000cP.s浆料放置24h，浆料的粘度与pH至无明显变化，将其在铝箔上进行涂布，表观良好，无露箔及气泡生成。浆料的粘度及pH数据如下表3所示：
表3浆料的粘度及pH数据变化
| 时间 | 0h | 1h | 4h | 24h |
| 粘度 | 5000 | 6200 | 8800 | 9800 |
| pH | 8 | 8.8 | 9.6 | 10.4 |
采用市面上常用的锂离子电池用PAA类水性粘合剂(市售，请补充厂家名称)制备正极三元材料浆料：取PAA粘合剂(15％固含)的粘合剂40g以及水85g缓慢搅拌5min，加入导电剂Super P 4g高速搅拌100min，然后加入188g正极三元材料(NCA811)高速搅拌100min，制得的正极三元材料浆料固含为68％，粘度为5000cP.s浆料放置24h,测试其pH值变化如表4所示。
表4PAA粘合剂三元材料浆料的粘度及pH数据变化
| 时间 | 0h | 1h | 4h | 24h |
| 粘度 | 5000 | 8200 | 10000 | 16800 |
| pH | 9.3 | 10 | 11.3 | 11.4 |
浆料放置完毕，在铝箔上涂布会有气体产生，铝箔腐蚀严重。如表3与表4对比可知，利用实施例3中所制备的水性粘合剂所制备的浆料放置24h后，粘度，pH值的变化均明显小于市售PAA粘合剂，具有显著性。可见，对比目前市场上锂离子电池正极水性粘合剂主流PAA粘合剂,实施例3中所制备的水性粘合剂能显著抑制三元材料浆料pH的变化，可在一定存放周期内抑制pH的增大。
实施例5
本实施例中，将2份的聚丙烯酸钠溶于反应釜中，待聚丙烯酸钠完全溶解后依次加入0.6份的2-烯丙基醚3-羟基丙烷-1-磺酸盐，30份的丙烯酸丁酯、10份的亚甲基丁二酸以及10份的醋酸乙烯，升高温度至70℃，快速加入0.5份的过硫酸钾溶液，反应200min，制备前段聚合物；待反应完成后保持温度不变快速加入10份的醋酸乙烯以及0.1份的过硫酸钾溶液，保持70℃恒温反应80min，待反应完成后将25份的丙烯酸丁酯、10份的醋酸乙烯以及5份的亚甲基丁二酸在0.3份的十八烷基琥珀酸钠制成预乳液，将预乳液与0.3份的过硫酸钾溶液缓慢滴加，200min滴加完毕，升高温度至74℃，保温200min；即制得锂离子电池三元材料用水性粘合剂，粘合剂粘度在8000-12000cP.s，粘合剂固含为15％。
实施例6
将实施例5制备的粘合剂40g以及水85g缓慢搅拌5min，加入导电剂Super P 4g高速搅拌100min，然后加入188g正极三元材料(NCA811)高速搅拌100min，制得的正极三元材料浆料固含为66％，粘度为5000cP.s浆料放置24h，浆料的粘度与pH至无明显变化，将其在铝箔上进行涂布，表观良好，无露箔及气泡生成。浆料的粘度及pH数据如下表5所示：
表5浆料的粘度及pH数据变化
| 时间 | 0h | 1h | 4h | 24h |
| 粘度 | 5000 | 5800 | 7000 | 8100 |
| PH | 8.2 | 8.6 | 9 | 9.3 |
如表5所示，将其与表4进行比较可见利用实施例5中所制备的水性粘合剂所制备的浆料放置24h后，粘度，pH值的变化均明显小于市售PAA粘合剂，具有显著性，对比目前市场上锂离子电池正极水性粘合剂主流PAA粘合剂，实施例5中所制备的水性粘合剂能显著抑制三元材料浆料pH的变化，可在一定存放周期内抑制pH的增大。
本申请实施例中提供的水性粘合剂能够配合锂离子电池高能量密度的发展，例如NCA523以及NCA811等三元材料的快速发展，其能够适应不同NCA比例的锂离子电池三元材料，能够调节水性锂离子电池三元材料浆料的pH，能够适应高碱性环境下的制浆及涂布工艺，具有广阔的应用前景。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换等，均应包含在本发明的保护范围之内。
Claims (8)
1.一种水性粘合剂，其特征在于，通过以下方法制备，所述方法包括如下步骤：
（1）在保护胶的作用下，将含羧基的功能单体、醋酸乙烯单体以及丙烯酸酯单体混合进行前段共聚合形成粘合剂前段；
（2）前段聚合物反应结束，加入醋酸乙烯单体进行中段聚合形成粘合剂中段；
（3）待中段聚合结束，滴加预先将含羧基的功能单体、醋酸乙烯单体以及丙烯酸酯单体制备形成的预乳液，使反应完全形成粘合剂后段；
其中，所述含有羧基的功能单体为含有羧基和不饱和键的化合物。
2.如权利要求1所述的水性粘合剂，其特征在于，所述粘合剂前段或后段中含有羧基的功能单体质量占比为5%-50%。
3.如权利要求1所述的水性粘合剂，其特征在于，所述粘合剂前段或后段中醋酸乙烯与所述共聚物的质量占比10%-40%。
4.如权利要求1-3中任一项所述的水性粘合剂，其特征在于，所述含羧基的功能单体选自甲基丙烯酸、丙烯酸、马来酸、衣康酸或马来酸酐中的一种或多种。
5.如权利要求1-3中任一项所述的水性粘合剂，其特征在于，所述丙烯酸酯单体选自丙烯酸乙酯、丙烯酸丁酯、丙烯酸正/异辛酯、丙烯酸月桂酯、甲基丙烯酸聚乙二醇单甲醚、甲基丙烯酸甲酯和甲基丙烯酸羟乙酯中的一种或多种。
6.如权利要求1-5中任一项所述的水性粘合剂的制备方法，其特征在于，包括：
（1）在保护胶的作用下，将含羧基的功能单体、部分醋酸乙烯单体以及丙烯酸酯单体混合进行前段聚合；
（2）前段聚合物反应结束，加入醋酸乙烯单体进行中段聚合；
（3）待中段聚合结束，加入预先将含羧基的功能单体、醋酸乙烯单体以及丙烯酸酯单体形成的预乳液，使反应完全。
7.如权利要求6所述的制备方法，其特征在于，所述保护胶包括但不限于聚丙烯酰胺、聚丙烯酸盐、聚乙烯醇、羟乙基纤维素或羧甲基纤维素中的一种或多种。
8.权利要求1-5中任一项所述的水性粘合剂，或权利要求6或7所制备的水性粘合剂在锂离子电池三元材料中的应用。
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